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(3-Hydroxypropyl)triphenylphosphonium bromide → (1S,3aS,5S,7aR)-1-acetoxymethyl-5-[(E)-4-hydroxy-1-butenyl)-7a-methylperhydro-inden-3a-ol

HRID 725185
ノート
印刷プレビュー

反応式

HRID 725185 の反応式
[Br-].[OH:2][CH2:3][CH2:4][CH2:5][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.C([Li])CCC.[C:30]([O:33][CH2:34][C@@H:35]1[C@:43]2([CH3:44])[C@@:38]([OH:47])([CH2:39][C@@H:40]([CH:45]=O)[CH2:41][CH2:42]2)[CH2:37][CH2:36]1)(=[O:32])[CH3:31]>C1COCC1.CCCCCC>[C:30]([O:33][CH2:34][C@@H:35]1[C@:43]2([CH3:44])[C@@:38]([OH:47])([CH2:39][C@@H:40](/[CH:45]=[CH:5]/[CH2:4][CH2:3][OH:2])[CH2:41][CH2:42]2)[CH2:37][CH2:36]1)(=[O:32])[CH3:31]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11025793(3-Hydroxypropyl)triphenylphosphonium bromideHCID 57272999(1S,3aS,5S,7aR)-1-acetoxymethyl-3a-hydroxy-5-formyl-7a-methylperhydroindeneHCID 178418339Butyllithium

生成物 1

HCID 70051238(1S,3aS,5S,7aR)-1-acetoxymethyl-5-[(E)-4-hydroxy-1-butenyl)-7a-methylperhydro-inden-3a-ol収率 59.8%

試薬・触媒・溶媒 2

HCID 8028
Tetrahydrofuran
溶媒
2 回
HCID 8058Hexane溶媒

反応条件

温度
-25 °C

実験手順

To a suspension of 23.0 g of (3-hydroxypropyl)triphenylphosphonium bromide in 280 ml of anhydrous THF cooled at -25° C., 36.0 ml of 1.6N n-butyllithium in n-hexane were added dropwise under a nitrogen atmosphere and the mixture was stirred at -25° C. for 1 hr. A solution of 3.20 g of (1S,3aS,5S,7aR)-1-acetoxymethyl-3a-hydroxy-5-formyl-7a-methylperhydroindene in 32 ml of anhydrous THF was added and the reaction mixture was kept at -20° C. for 4 hrs, then warmed to room temperature and stirred for 3 hrs. The mixture was diluted with 5% aqueous NaH2PO4.H2 O, concentrated under reduced pressure and extracted with ethyl acetate. The organic layer was dried over sodium sulfate and evaporated to dryness under reduced pressure. The residue was purified by flash-chromatography (SiO2) with n-hexane/chloroform/acetone 6:2:2 to give 2.23 g of (1S,3aS,5S,7aR)-1-acetoxymethyl-5-[(E)-4-hydroxy-1-butenyl)-7a-methylperhydro-inden-3a-ol from which, by reaction with tert-butyldimethyl-chlorosilane, following the procedure, described in Prepn. 1, 2.94 g of (1S,3aS,5S,7aR)-1-acetoxymethyl-5-[(E)-4-tert-butyldimethylsilyl-oxy-1-butenyl)-7a-methylperhydroinden-3a-ol were obtained as a white foam.

後処理

  1. waitthe reaction mixture was kept at -20° C. for 4 hrs
  2. temperaturewarmed to room temperature
  3. stirringstirred for 3 hrs
  4. concentrationH2 O, concentrated under reduced pressure
  5. extractionextracted with ethyl acetate
  6. dry with materialThe organic layer was dried over sodium sulfate
  7. customevaporated to dryness under reduced pressure
  8. customThe residue was purified by flash-chromatography (SiO2) with n-hexane/chloroform/acetone 6:2:2

出典と根拠

ORDレコード
ord-7105808fdd9548c9963b4ade6f7eadda
出典データセット
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05705531

反応ノート

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